Potassium Carbonate → 1-(2,2,2-Trifluoroethyl)thiourea

HRID 1191075노트

반응식

HRID 1191075 반응식
C([NH:9][C:10]([NH:12][CH2:13][C:14]([F:17])([F:16])[F:15])=[S:11])(=O)C1C=CC=CC=1.C(=O)([O-])[O-].[K+].[K+]>CO.O>[F:15][C:14]([F:17])([F:16])[CH2:13][NH:12][C:10]([NH2:9])=[S:11]

참가 물질

5

반응물 2

HCID 11430Potassium CarbonateHCID 58495575HCID 58495575, 화합물

생성물 1

HCID 202028121-(2,2,2-Trifluoroethyl)thiourea수율 66%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

Slurry 1-benzoyl-3-(2,2,2-trifluoroethyl)-thiourea (5.5 g, 21.2 mmol) and potassium carbonate (11.7 g, 84.7 mmol) in methanol (180 mL) and water (40 mL). Stir the mixture at room temperature for 16 h. Concentrate the solution in vacuo to a paste. Triturate with hot water (20 mL, 60° C.), filter off the solids, wash with water (20 mL, 25° C.) and hexane (excess). Collect the solids, slurry in EtOAc and concentrate in vacuo twice to remove residual water. Dry the material in a vacuum oven at 45° C. for 16 h to obtain the desired intermediate as an off-white solid (2.2 g, 66%). MS (ES+) m/z: 159.1 (M+H)+.

후처리

  1. concentrationConcentrate the solution in vacuo to a paste
  2. customTriturate with hot water (20 mL, 60° C.)
  3. filtrationfilter off the solids
  4. washwash with water (20 mL, 25° C.) and hexane (excess)
  5. customCollect the solids, slurry in EtOAc
  6. concentrationconcentrate in vacuo twice
  7. customto remove residual water
  8. customDry the material in a vacuum oven at 45° C. for 16 h

출처 및 근거

ORD 기록
ord-da0721c021574b16ad5c902124d32dfd
출처 데이터셋
uspto-grants-2014_03
특허 번호
US08680091B2

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